Band 38, Heft 1-2

Six new diorganotin (IV) complexes, [Ph 2 Sn(Pr-ACDA) 2 ] 1 , [Bu 2 Sn(Pr-ACDA) 2 ] 2 , [Ph 2 Sn(Bz-ACDA) 2 ] 3 , [Bu 2 Sn(Bz-ACDA) 2 ] 4 , [Me 2 Sn(Bz-ACDA) 2 ] 5 , [t-Bu 2 Sn(Bz-ACDA) 2 ] 6 are reported (where ACDA is the 2-amino-1-cyclopentene-1-carbodithioic anion). The diorganotin complexes were prepared from reactions between sodium N-propyl and N-benzyl-2-amino-1-cyclopentene-1-carbodithioate with R 2 SnCl 2 (R=Ph, Bu, Me, tBu) in a 2:1 ratio. All complexes were characterized by elemental analysis, IR, multinuclear NMR ( 1 H, 13 C, and 119 Sn), FAB + mass spectrometry and in the case of 2 , 3 and 5 by single-crystal X-ray diffraction. Both solution and solid state studies show that dithioacid ligands are coordinated to tin in an aniso-bidentate manner. In all complexes coordination takes place only through the carbodithioate moieties. 119 Sn NMR data indicate pentacoordination of tin in solution. The tin coordination geometry, in all three structures is a highly distorted octahedral geometry, where tin is bonded to the four sulfur atoms of the two aniso-bidentate carbodithioate ligands in the equatorial plane and the organic substituents on tin atom in trans -positions. In addition, the crystal structures show the presence of N-H…S hydrogen bonding contacts.

Good-quality single crystals of polydistrontiumdimalatepentahydrate, a two-dimensional porous metal-organic framework, were successively grown by gel diffusion technique. Sodium metasilicate was used for gel preparation. Single crystal X-ray diffraction analyses showed that the compound crystallizes in triclinic space group P-1. The functional groups present in the crystals were identified by Fourier transform-infrared analysis. Elemental, powder X-ray diffraction and UV-visible spectral analyses of the compound were also performed. Thermal stability of the grown crystals was analyzed by thermogravimetry. Dielectric analyses of the title compound were conducted at room temperature in the frequency range of 400 Hz–4 MHz.

Reactions of aluminium isopropoxide with 2-(o-hydroxyphenyl)-benzoxazole (pbox H ) and salicylidene-4-chloroaniline (spca H ) in different molar ratios in benzene solution afforded the complexes of the types [(μ-OPr i ) 2 Al 2 (pbox) 2 (OPr i ) 2 ] 1 , [Al(OPr i )(pbox) 2 ] 2 , [Al(pbox) 3 ] 3, [(μ-OPr i ) 2 Al 2 (spca) 2 (OPr i ) 2 ] 4 , [Al(OPr i )(spca) 2 ] 5 and [Al(spca) 3 ] 6 . All these colored solid complexes are soluble in common organic solvents and were characterized by elemental (C, H, N and Al) analysis, spectroscopic [IR ( 1 H, 13 C and 27 Al) NMR] and mass spectrometric studies. On the basis of these studies, plausible structures have been tentatively proposed for these complexes.

Two triorganotin carboxylates of 1-methyl-1 H -imidazole-4-carboxylic acid (HL), Cy 3 SnL and C 6 H 5 C(CH3) 2 CH 2 SnL, have been prepared by the reaction of the ligand with tricyclohexyltin hydroxide and fenbutatin oxide, respectively. The complexes were characterized by 1 H NMR, infrared, and elemental analysis. The molecular structure of complex 1 was determined by using a single-crystal X-ray diffraction analysis. Preliminary bioassay indicated complex 1 exhibiting good and broad-spectrum fungicidal activities.

The self-assembly of [Zn(L)(H 2 O) 2 ]·Cl 2 and sodium 1,3,5-cyclohexanetricarboxylate yields a 3D hydrogen-bonded polymer [Zn(L)(H 2 chtc - )]H 2 chtc - ·H 2 O ( 1 ) (L=3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0 1.18 ,0 7.12 ]docosane, H 3 chtc=1,3,5-cyclohexanetricarboxylic acid). Complex 1 is characterized by X-ray crystallography, spectroscopy and thermogravimetric analyzer. The coordination geometry around the zinc(II) atom is a distorted square-pyramidal with four nitrogen atoms of the macrocycle occupying the basal sites and one carboxylate oxygen atom of the H 2 chtc - ligand at the apical position. The compound crystallizes in the monoclinic system p 2 1 /c with a =8.5287(8), b =39.241(3), c =12.6135(11) Å, β (°)= 104.525(6)°, V =4086.5(6) Å 3 , Z =4. The IR spectrum and the TGA behavior of the complex are significantly affected by the 1,3,5-cyclohexanetricarboxylic acid.

A new Cd(II) complex, [Cd(PMBP) 2 (CH 3 OH) 2 ] (PMBP = 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone), has been synthesized and characterized by elemental analysis, IR spectroscopy, thermal gravimetric analysis, fluorescence analysis, and X-ray single-crystal diffraction. In the complex, a slightly distorted octahedral geometry of cadmium ion is coordinated by six oxygen atoms, and the cadmium ion locates in the center position. The complex is a monomeric species, which is extended into 2D supramolecular architecture by strong intermolecular hydrogen bonds. Moreover, the intramolecular hydrogen bonds and C-H···π interactions are also found in the complex so that the 2D supramolecular network is consolidated.

Zero-valent antimony and antimony oxide were deposited on graphene oxide by the recently introduced peroxide deposition route. The antimony@graphene oxide (GO) anode exhibits a charging capacity of 340 mAh g -1 with excellent stability at a current rate of 250 mA g -1 after 50 cycles of lithiation, which is superior to all other forms of antimony anodes that have been reported thus far. The electrode also exhibits a good rate performance, with a capacity of 230 and 180 mAh g -1 at a rate of 500 and 1000 mA g -1 , respectively. We attribute the superior performance of the antimony@GO anodes to our coating protocol, which provides a thin layer of nanometric antimony coating on the graphene oxide, and to a small amount of antimony oxide that is left in the anode material after heat treatment and imparts some flexibility. The efficient charge distribution by the large surface area of reduced GO and the expansion buffering of the elastic graphene sheets also contributed to the superior stability of the anode.

The synthesis of cyclic disilene 10 was attempted by photolysis of 2-alkynyltrisilane 9 . As a result, silylsilylene 14 was generated, along with the elimination of the alkynylsilane moiety, in the photolysis of 2-alkynyltrisilane 9 , similar to the photolysis of alkynyldisilane. In addition, the product 14 trapped by triethylsilane underwent further photolysis to produce hydrosilylene 16 .

ZnCl 2 ·2H 2 NN(H)Bu t ·H 2 O contains a tetrahedral metal centre with two coordinated hydrazine ligands. Hydrogen bonds between the hydrazine and water, along with weaker intermolecular NH…Cl, OH…Cl and NH…O hydrogen bonds, generate an associated lattice.